Treatment of high-boiling coal-tar distillates for the production of resinous products



' a hard pitch, the highest boiling 'distillates' uses for the pitch beUNITED STATES PATENT OFFICE.

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ANIGNORS TO THE BAEBETT OOHPANY, A. CORPORATION TREATMENT OFHIGH-BOILING COAL-TAB DISTILM'I'EB 1'03 ll-HE PRODUCTION OF RESINOUS-PBODUCIS.

no Drawing. Application med October e7, 1010. Serial No. aaaaao. Toallaohom itmafi cmwem: Be it known t at, we (1) GEORGE C.

BAILEY, a citizen of. the Tlnited States, and (2) Fnux Bom'rmm a citizenof German residin at (1%VWoodclifi-on-Hudson, N. and (2' '170 est 89thSt., New York in the counties of (1) Hudson and (2) blew York and Statesof 1) New Jersey and (2) New York, have invented certain new and usefulIm rovements in Treatment 'of H h- 6 Boiling oal-Tar Distillates for theduction of Resinous Products, of which the following is a specification.

high boiling coal-tar distillates whereby new! products having valuablecharacteristies are obtained.

In the ordinary distillation of coal-tar to are the so-called greenoils, which contain the highly use 111 products anthracene and carbazol,as well as many other bodies less well known. Since the duction of,anthracene and carbazol entails the formation of much hard pitch it isdesirable that evelo ed. Besides the briqueting of coal, one o the usesfor this pitch is found in the production of itch coke, which is usefulas a valuable ubstitute for petroleum coke. It is not economical withthe usual type of coal-tar still to run the hard pitch to the cokingpoint, as the high heat necessary woul shorten the life of the stillvery materially, hence a s ecial type of retort is used to convert thehard itch into a coke, thereb introducing another step in the process 0dis tillin coal tar. During the coking process a big boiling distillatedistilsor sublimes oil from the hard itch at a high vapor temperature,which istillate may be readily collected. This distillate usuallyamounts to about two per cent. or more of the hard itch that isdistilled to produce the coke. e actual percentage'may vary depending toa certain extent upon the coal-tarpitc charged, the temperature, thetimeof running the distillation and the character of coal-tar distillationdepending upon the coal-tar source and the other factors.Similpeemcatlon of Lctten Patent.

lar distillates may Society for. Te'sting Materials.

solid to solid bitumen of hi h This invention relates to the treatmentof exposure to air.

resinous materials from the so ids an be obtained in the high fractions'obtaine from continuous coal-tar stills as well as from otherdistillations' such as gas circulation, vacuum distillation and others.These distillates are bituminous in character and may properly bereferred to as bltumen, within the standard definition of bitumen asgiven by the American They are semi-solid to solid at ordinaryatmospheric temperatures, boil at high temperatures, and will bereferred to in the claims as semiboiling point obtained from coal tar.his bitumen is often referred to as pitch resin"by those skilled in thisart. 1

The itch resin is usually a sticky orangecolore gummy mass which darkensupon When warmed to sli htly above C. it becomes fluid enoug to pourfrom one vessel to another. It possesses few properties in its originalstate which render it useful for such purposes as an ingredient forvarnish, or as resin or constituents and from our experiments we' havedeveloped methodsof se aratin the oils and have thereby produced new anduseful product's.

By experiment we have found that the resin obtained as above describedcould be distilled completely under a bi h vacuum and that certain ofthe disti'lates were harder than the original resin. We have found thatcertain solvents will dissolve Patented Oct. 5,1920.

art of the original pitch resin and leave hind solids which ,can becrystallized thereby obtaining a dry yellow powder. By

combining the two treatments 'we have worked out a moose whereby verytransparent hard resins may be obtained.

The following explanation will make the process understood. A quantityof the resin is warmed with a solvent, until the mass is quite fluid.For example, if toluene isused as the solvent, the proportions may beabout 1000 parts of resin to 120 arts of toluene. 1 The mass is thanallo to cool slowlyt until it reaches room temperature. It maypreferablybe cooled by running water or ice water. U on cooling, themass becomes item C. and over. These solids or crystals sometimes amountto about 8% of the original mamas was treated with the solvent,

.the amount of solids depending largely upon the nature of the originalresin.

The filtrate is then distilled to remove the solvent, after which theresidue is distilled under a high vacuum and various cuts are madeduring the distillation. The cuts in the distillation of the filtrateare made at various intervals degmnding upon the quality and character 0thedesired prodnote; For example, the solvent is first regained which isre-used in another extraction. Later, up to about 20 C. under anabsolute pressure of 8 mm. a heavy oil is obtained which does not solidiand may be returned to the creosote oils. rom 220 to about 275 yellowishgreases are obtained. From about 275 to about 400 C. under the aboveabsolute ressure trans arent red resins are obtained varying in egree ofhard ness as the tem erature increases. These resins may be re istilledif the first distillation does not give suitable products. The hardestresin may melt at C. to 100! by the same empirical methods as used totest the softening point of pitches. This resin is transparent and doesnot discolor upon standing exposedto air and light.

Furthermore a vacuum distillation may be made on the resin as receivedfrom! the coking retorts and the several cuts washed with suitablesolvents and these solutions again distilled or the various cuts fromthe vacuum distillation may be utilized as they are received from thevacuum still.

By any of these p resinous materials may be obtained which are quitehard w: little tendency to change color upon long standing. Thetransparent red resins have melting points of a range as wide or widerthan from about 40 C. to 100 (3. depending upon the temperature at whichthe cuts are made. These resins are comcoal tar with if solvent, filteriplea mixtures robabl of an not yet identified c emical y.

Samplesof these transparent red resins mixtures, rubber compounding,water proof ing mixtures and as a substitute for various waxes andresins.

Claims: 1. The herein describediprocess which comprises extracting'witha solvent, a semisolid to solid bitumen of high boili point obtainedfrom coal tar, separating t e solution removing the solvent from thesolution, distilling the residue under vacuum.

2. The ,herein described process which comprises extrwcti a semi-solidto solid bitumen of high boiling point obtained from distilling thesolvent from the filtrate, and distilling the residue under vacuum.

3. The herein described process which com rises extracting with asolvent, a semisoli to solid bitumen of high boiling oint obtained fromcoal tar filtering, disti ling the solvent from the filtrate, distillingthe residue under vacuum and separating the vacuum distillate intofractions having different boiling points.

4. The herein described process which com rises extracting with asolvent a semisoli to solid bitumen of high boiling int obtainedfromcoal tar, filtering, distilling the solvent from the filtrate,distilling the residue under vacuum, separating the distillate intofractions haviflgrdiflerent boilin points and redistilling one .or moreof said fractions under vacuum.

5. A transparent, red resin derived from a semi-solid to solid bitumenof hi h boiling point obtained from coal tar which does not darken uponex osure to air and light and which can be distilled under vacuumwithout substantial decom osition.

6. A transparent re resin derived from a semi-solid to solid bitumen ofhigh boiling point obtained from coal tar which melts above 40 C. andwhich can be distilled uniler vacuum without substantial decomposiion.

I. A transparent red resin derived from a semi-solid to solid bitumen ofhigh boiling point obtained from coal tar and containing carbon andhydrogen in substantially the proportion of 20 to l and which can bedistilled under vacuum without substantial de- 5 composition.

8. A hard, transparent, red resin derived from a semi-so1id to solidbitumen of high boiling point obtained from coal tar, which does notdarken upon exposure to air and 10 light, having a melting point above40 C.

containing carbon and hydrogen in substantially the proportion of 20 to1, and being partly soluble in petroleum naphthas and which can bedistilled under vacuum Without substantial decomposition.

In testimony whereof We aflix our signatures.

GEORGE C. BAILEY. FELIX BOETTNER.

It is hereby certified that in Letters Patent No. 1,355,103, grantedOctober 5,

of WoodcIift-on-Hudson, New

for an improvement in 1920, upon the application of George C. Bailey,Jersey, and Felix Boettner, of New York, N. 1., "Treatment ofHigh-Boiling Coal-Tar Distillates for the Production of ResinousProducts," an error appears in the printed specification requiringcorrection as follows: Page 2, line 34, for about 20 C." read obaut 2200.; and that the said Letters Patent should be read with this correctiontherein that the same may conform to the record of the case in thePatent Office.

Signed and sealed this 30th day of Novemher, A. D., 1920.

L. B. MANN,

Acting Commissioner of Patmfl.

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